WO2022145340A1 - Plaque de verre renforcée et procédé de production associé - Google Patents

Plaque de verre renforcée et procédé de production associé Download PDF

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WO2022145340A1
WO2022145340A1 PCT/JP2021/047907 JP2021047907W WO2022145340A1 WO 2022145340 A1 WO2022145340 A1 WO 2022145340A1 JP 2021047907 W JP2021047907 W JP 2021047907W WO 2022145340 A1 WO2022145340 A1 WO 2022145340A1
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glass plate
tempered glass
content
plate according
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PCT/JP2021/047907
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English (en)
Japanese (ja)
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健 結城
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日本電気硝子株式会社
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Priority to KR1020237022954A priority Critical patent/KR20230128293A/ko
Priority to JP2022573039A priority patent/JPWO2022145340A1/ja
Priority to CN202180087025.8A priority patent/CN116745247A/zh
Publication of WO2022145340A1 publication Critical patent/WO2022145340A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements

Definitions

  • the present invention relates to a tempered glass plate and a method for manufacturing the same, and particularly to a tempered glass plate suitable for a cover glass of a touch panel display such as a mobile phone, a digital camera, and a PDA (mobile terminal) and a method for manufacturing the tempered glass plate.
  • a tempered glass plate that has been ion-exchanged is used as a cover glass for a touch panel display (see Patent Documents 1 to 3 and Non-Patent Document 1). ..
  • Lithium aluminosilicate glass is advantageous in obtaining deep stress depths.
  • a tempered glass plate made of lithium aluminosilicate glass is immersed in a molten salt containing NaNO 3 and the Li ions in the glass and the Na ions in the molten salt are ion-exchanged, the tempered glass has a deep stress depth. You can get a board.
  • the compressive stress value of the compressive stress layer may become too small.
  • the glass composition is designed so as to increase the compressive stress value of the compressive stress layer, there is a risk that the chemical stability will decrease.
  • an alumina-based refractory or a zirconia-based refractory is used as the refractory of the molded body. Since the conventional lithium aluminosilicate glass has low compatibility with these molded refractories (particularly alumina-based refractories), bubbles and bumps are likely to occur, and there is a risk that plate molding becomes difficult.
  • the present invention has been made in view of the above circumstances, and its technical problems are tempered glass having good compatibility with a molded refractory, excellent chemical stability, and being hard to be damaged when dropped. Is to provide a board.
  • the reinforced glass plate of the present invention is a reinforced glass plate having a compressive stress layer on the surface, and the glass composition is SiO 2 55 to 80%, Al 2 O 3 11 to 25%, B 2 O 3 in terms of glass composition.
  • [X] refers to the molar% content of the X component.
  • [Li 2 O] refers to the molar% content of Li 2 O.
  • [Na 2 O] refers to the molar% content of Na 2 O.
  • [K 2 O] refers to the molar% content of K 2 O.
  • [Al 2 O 3 ] refers to the mol% content of Al 2 O 3 .
  • [MgO] refers to the mol% content of MgO. ([Li 2 O] + [Na 2 O] + [K 2 O]) / [Al 2 O 3 ] is the sum of Li 2 O, Na 2 O and K 2 O and the content of Al 2 O 3 . Refers to the value divided by.
  • [MgO] / [Al 2 O 3 ] refers to a value obtained by dividing the content of MgO by the content of Al 2 O 3 .
  • the tempered glass plate of the present invention preferably has a Li 2 O content of 11.4 mol% or less.
  • the tempered glass plate of the present invention preferably has a P2O5 content of 0.001 mol% or more .
  • the tempered glass plate of the present invention preferably has a K2O content of 0.001 mol% or more .
  • the tempered glass plate of the present invention preferably has a B2O3 content of 0.4 mol% or more .
  • the tempered glass plate of the present invention preferably has a Cl content of 0.02 mol% or more.
  • the tempered glass plate of the present invention does not cause devitrification when it is brought into contact with an alumina refractory at a temperature equal to or higher than 10 4.5 dPa ⁇ s for 48 hours.
  • the tempered glass plate of the present invention is characterized in that the softening point is 920 ° C. or lower.
  • the compressive stress value on the outermost surface of the compressive stress layer is preferably 200 to 1200 MPa.
  • the stress depth of the compressive stress layer is preferably 50 to 200 ⁇ m.
  • the "compressive stress value on the outermost surface” and the “stress depth” were measured from a phase difference distribution curve observed using, for example, a scattered light photoelastic stress meter SLP-1000 (manufactured by Orihara Seisakusho Co., Ltd.). Point to a value.
  • the stress depth refers to the depth at which the stress value becomes zero.
  • the refractive index of each measurement sample is 1.51 and the optical elastic constant is 29.0 [(nm / cm) / MPa].
  • the tempered glass plate of the present invention preferably has a temperature of less than 1680 ° C. at a high temperature viscosity of 10 2.5 dPa ⁇ s.
  • the "temperature at a high temperature viscosity of 10 2.5 dPa ⁇ s" can be measured by, for example, a platinum ball pulling method.
  • the tempered glass plate of the present invention has an overflow confluence surface at the central portion in the plate thickness direction.
  • the "overflow down draw method” overflows the molten glass from both sides of the refractory of the molded body, and while merging the overflowed molten glass at the lower end of the refractory of the molded body, stretch-molds the glass plate downward. It is a manufacturing method.
  • the tempered glass plate of the present invention is preferably used for the cover glass of the touch panel display.
  • the tempered glass plate of the present invention preferably has a Fe 2 O 3 content of 0.001 to 0.1 mol%.
  • the tempered glass plate of the present invention preferably has a TiO 2 content of 0.001 to 0.1 mol%.
  • the tempered glass plate of the present invention preferably has a SnO 2 content of 0.001 mol% or more.
  • the tempered glass plate of the present invention has a bent stress profile in the thickness direction.
  • the tempered glass plate of the present invention has at least a first peak, a second peak, a first bottom, and a second bottom in the stress profile in the thickness direction.
  • the glass composition is mol%, SiO 2 55 to 80%, Al 2 O 3 11 to 25%, B 2 O 30 to 10%, Li 2 O 0. .02 to 15%, Na 2 O 1 to 21%, K 2 O 0 to 10%, MgO 0.01 to 5 %, P 2 O 50 to 15%, SnO 20 to 0.30% , Mole ratio [MgO] / [Al 2 O 3 ] ⁇ 0.20, and molar ratio ([Li 2 O] + [Na 2 O] + [K 2 O]) / [Al 2 O 3 ] ⁇
  • the reinforcing glass plate of the present invention has a molar composition of SiO 2 55 to 80%, Al 2 O 3 11 to 25%, B 2 O 30 to 10%, and Li 2 O 0.02 to 15 in terms of the glass composition. %, Na 2 O 1 to 21%, K 2 O 0 to 10%, MgO 0.01 to 5 %, P 2 O 50 to 15%, SnO 20 to 0.30%, and the molar ratio [ MgO] / [Al 2 O 3 ] ⁇ 0.20 and molar ratio ([Li 2 O] + [Na 2 O] + [K 2 O]) / [Al 2 O 3 ] ⁇ 0.80. It is characterized by being.
  • the tempered glass plate (strengthening glass plate) of the present invention has a glass composition of mol%, SiO 2 55 to 80%, Al 2 O 3 11 to 25%, B 2 O 30 to 10%, Li 2 O. Contains 0.02 to 15%, Na 2 O 1 to 21%, K 2 O 0 to 10%, MgO 0.01 to 5 %, P 2 O 50 to 15%, SnO 20 to 0.30%
  • the reasons for limiting the content range of each component are shown below. In the description of the content range of each component, the% indication indicates mol% unless otherwise specified.
  • SiO 2 is a component that forms a network of glass. If the content of SiO 2 is too small, it becomes difficult to vitrify, and the coefficient of thermal expansion becomes too high, so that the thermal impact resistance tends to decrease. Therefore, the preferred lower limit range of SiO 2 is 55% or more, 57% or more, 59% or more, and particularly 61% or more. On the other hand, if the content of SiO 2 is too large, the meltability and moldability tend to decrease, and the coefficient of thermal expansion becomes too low, making it difficult to match the coefficient of thermal expansion of the peripheral material. Therefore, the preferred upper limit range of SiO 2 is 80% or less, 70% or less, 68% or less, 66% or less, 65% or less, and particularly 64.5% or less.
  • Al 2 O 3 is a component that enhances ion exchange performance, and is also a component that enhances strain point, Young's modulus, fracture toughness, and Vickers hardness. Therefore, the suitable lower limit range of Al 2 O 3 is 11% or more, 11.4% or more, 11.6% or more, 11.8% or more, 12% or more, 12.5% or more, 13% or more, 13. 5% or more, 14% or more, 14.4% or more, 15% or more, 15.3% or more, 15.6% or more, 16% or more, 16.5% or more, 17% or more, 17.2% or more, 17.5% or more, 17.8% or more, 18% or more, 18% or more, 18.3% or more, especially 18.5% or more, 18.6% or more, 18.7% or more, 18.8% or more Is.
  • the preferred upper limit of Al 2 O 3 is 25% or less, 21% or less, 20.5% or less, 20% or less, 19.9% or less, 19.5% or less, 19.0% or less, especially 18 It is 9.9% or less. If the content of Al 2 O 3 having a large influence on the ion exchange performance is set in a suitable range, it becomes easy to form a profile having a first peak, a second peak, a first bottom, and a second bottom.
  • B 2 O 3 is a component that lowers the high-temperature viscosity and density, stabilizes the glass, makes it difficult for crystals to precipitate, and lowers the liquidus temperature. Furthermore, it is a component that enhances the binding force of oxygen electrons by cations and lowers the basicity of glass. If the content of B 2 O 3 is too small, the stress depth in the ion exchange between Li ions contained in the glass and Na ions in the molten salt becomes too deep, and as a result, the compressive stress value (CS) of the compressive stress layer becomes too deep. Na ) tends to be small. In addition, the glass may become unstable and the devitrification resistance may decrease.
  • the suitable lower limit range of B 2 O 3 is 0% or more, 0.10% or more, 0.12% or more, 0.15% or more, 0.18% or more, 0.20% or more, 0.23%. 0.25% or more, 0.27% or more, 0.30% or more, 0.35% or more, 0.38% or more, 0.4% or more, 0.42% or more, 0.45% or more, 0.5% or more, 0.6% or more, 0.7% or more, 0.8% or more, 0.9% or more, especially 1% or more.
  • the preferred upper limit range of B 2 O 3 is 10% or less, 9.5% or less, 9% or less, 8.5% or less, 8% or less, 7.5% or less, 7% or less, 6% or less, 5.5% or less, 5% or less, 4% or less, 3.8% or less, 3.5% or less, 3.3% or less, 3.2% or less, 3.1% or less, 3% or less, 2.
  • B 2 O 3 is set in a suitable range, it becomes easy to form a profile having a first peak, a second peak, a first bottom, and a second bottom.
  • Li 2 O is an ion exchange component, and is an essential component for ion exchange between Li ions contained in glass and Na ions in a molten salt to obtain a deep stress depth. Further, Li 2 O is a component that lowers the high-temperature viscosity, enhances meltability and moldability, and is a component that enhances Young's modulus. Therefore, the suitable lower limit range of Li 2 O is 0.02% or more, 0.03% or more, 0.1% or more, 0.5% or more, 1% or more, 2% or more, 3% or more, 4% or more. 5% or more, 5.5% or more, 6.5% or more, 7% or more, 7.3% or more, 7.5% or more, 7.8% or more, especially 8% or more.
  • the preferred upper limit of Li 2 O is 15% or less, 13% or less, 12% or less, 11.5% or less, 11.4% or less, 11.3% or less, 11.2% or less, 11.1 % Or less, 11% or less, 10.5% or less, less than 10%, especially 9.9% or less, 9% or less, 8.9% or less.
  • Na 2 O is an ion exchange component, and is a component that lowers high-temperature viscosity and enhances meltability and moldability. Further, Na 2 O is a component that enhances devitrification resistance, and in particular, is a component that suppresses devitrification caused by a reaction with an alumina-based refractory. Therefore, the preferred lower limit range of Na 2 O is 1% or more, 2% or more, 3% or more, 4% or more, 5% or more, 6% or more, 7% or more, 7.5% or more, 8% or more, 8 It is 5.5% or more, 8.8% or more, especially 9% or more.
  • the preferred upper limit range of Na 2 O is 21% or less, 20% or less, 19% or less, particularly 18% or less, 15% or less, 13% or less, 11% or less, and particularly 10% or less.
  • K 2 O is a component that lowers high-temperature viscosity and enhances meltability and moldability. However, if the content of K 2 O is too large, the coefficient of thermal expansion becomes too high, and the thermal impact resistance tends to decrease. In addition, the compressive stress value on the outermost surface tends to decrease. Therefore, the preferred upper limit range of K2O is 10 % or less, 7% or less, 6% or less, 5% or less, 4% or less, 3% or less, 2% or less, 1.5% or less, 1% or less, 1% or less. Less than%, 0.5% or less, especially less than 0.1%.
  • the suitable lower limit range of K2O is 0 % or more, 0.001% or more, 0.003% or more, 0.005% or more, 0.007% or more, 0.01% or more, 0.02% or more, 0.03% or more, 0.05% or more, 0.08% or more, 0.1% or more, 0.3% or more, especially 0.5% or more. ..
  • the molar ratio [MgO] / [Al 2 O 3 ] is preferably 0.20 or less, 0.19 or less, 0.18 or less, 0.17 or less, 0.16 or less, 0.15 or less, 0.12 or less. In particular, it is 0.10 or less. If [MgO] / [Al 2 O 3 ] is too large, devitrification lumps are likely to occur when the molded refractory (particularly alumina-based refractory) comes into contact with the refractory, and the quality of the reinforcing glass plate deteriorates. There is a risk.
  • the lower limit of the molar ratio [MgO] / [Al 2 O 3 ] is not particularly limited, but is substantially 0.01 or more, 0.02 or more, 0.03 or more, 0.04 or more, 0.05 or more. , 0.07 or more, especially 0.08 or more.
  • the molar ratio ([Li 2 O] + [Na 2 O] + [K 2 O]) / [Al 2 O 3 ] is preferably 0.80 or more, 0.81 or more, 0.82 or more, 0.83. 0.84 or more, 0.85 or more, 0.86 or more, 0.87 or more, 0.88 or more, 0.89 or more, 0.90 or more, 0.95 or more, 0.97 or more, 0.98 These are 0.99 or more, 1.0 or more, 1.1 or more, 1.2 or more, and particularly 1.3 or more. If the molar ratio ([Li 2 O] + [Na 2 O] + [K 2 O]) / [Al 2 O 3 ] is too small, the efficiency of ion exchange tends to decrease.
  • the molar ratio ([Li 2 O] + [Na 2 O] + [K 2 O]) / [Al 2 O 3 ] is preferably 2.0 or less, 1.8 or less, 1.7 or less, 1 6.6 or less, 1.5 or less, 1.4 or less, especially 1.3 or less.
  • Molar ratio ([SiO 2 ] + [B 2 O 3 ] + [P 2 O 5 ]) / ((100 x [SnO 2 ]) x ([Al 2 O 3 ] + [Li 2 O] + [Na 2 ] O] + [K 2 O] + [MgO] + [CaO] + [BaO] + [SrO] + [ZnO])) is preferably 0.15 or more, 0.20 or more, 0.22 or more, 0.
  • the upper limit of O] + [K 2 O] + [MgO] + [CaO] + [BaO] + [SrO] + [ZnO])) is not particularly limited, but is preferably 40.0 or less, 20.0 or less, 10.0 or less, 8.0 or less, 5.0 or less, 4.0 or less, 3.0 or less, 2.0 or less, 1.8 or less, 1.5 or less, 1.2 or less, 1.0 or less, It is 0.90 or less, 0.80 or less, and particularly 0.70 or less.
  • the molar ratio [Li 2 O] / ([Na 2 O] + [K 2 O]) is preferably 0.4 to 1.0, 0.5 to 0.9, and particularly 0.6 to 0.8. be. If the molar ratio [Li 2 O] / ([Na 2 O] + [K 2 O]) is too small, there is a risk that the ion exchange performance cannot be fully exhibited. In particular, the efficiency of ion exchange between Li ions contained in the glass and Na ions in the molten salt tends to decrease.
  • MgO is a component that lowers high-temperature viscosity to improve meltability and moldability, and increases strain points and Vickers hardness.
  • MgO has a large effect of improving ion exchange performance. It is an ingredient.
  • the suitable content of MgO is 0.01-5%, 0.05-5%, 0.02-5%, 0.1-6%, 0.2-5%, 0.5-5%. , 0.7 to 4.5%, 1.0 to 4.0%, 1.0 to 3%, 1.0 to 2.5%, especially 1.0 to 2%.
  • P 2 O 5 is a component that enhances the ion exchange performance, and is a component that particularly deepens the stress depth. Furthermore, it is a component that improves acid resistance. Furthermore, it is a component that enhances the binding force of oxygen electrons by cations and lowers the basicity of glass. If the content of P 2 O 5 is too small, there is a risk that the ion exchange performance cannot be fully exhibited. In particular, the efficiency of ion exchange between Na ions contained in the glass and K ions in the molten salt tends to decrease, and the stress depth (DOL_ZERO K ) of the compressive stress layer tends to decrease. In addition, the glass may become unstable and the devitrification resistance may decrease.
  • the suitable lower limit range of P 2 O 5 is 0% or more, 0.001% or more, 0.005% or more, 0.01% or more, 0.02% or more, 0.03% or more, 0.05%.
  • the stress depth in the ion exchange between the Li ion contained in the glass and the Na ion in the molten salt becomes too deep, and as a result, the compressive stress value (CS Na ) of the compressive stress layer tends to be small. Therefore, the preferred upper limit range of P 2 O 5 is 15% or less, 10% or less, 8% or less, 7% or less, 6% or less, 5% or less, 4.9% or less, and 4.8% or less. If the content of P 2 O 5 is in a suitable range, it becomes easy to form a non-monotonic profile.
  • SnO 2 is a clarifying agent and a component that enhances ion exchange performance, but if the content thereof is too large, the devitrification resistance tends to decrease. Therefore, the suitable lower limit range of SnO 2 is 0% or more, 0.001% or more, 0.002% or more, 0.005% or more, 0.007% or more, particularly 0.010% or more, and a suitable upper limit.
  • the range is 0.30% or less, 0.27% or less, 0.25% or less, 0.20% or less, 0.18% or less, 0.15% or less, 0.12% or less, 0.10% or less, 0.09% or less, 0.08% or less, 0.07% or less, 0.06% or less, 0.05% or less, 0.047% or less, 0.045% or less, 0.042% or less, 0. 040% or less, 0.038% or less, 0.035% or less, 0.032% or less, 0.030% or less, 0.025% or less, 0.020% or less, particularly 0.015% or less.
  • Cl is a clarifying agent.
  • the bubble diameter in the glass is likely to increase, and the clarification effect is likely to be exhibited.
  • suitable lower limit ranges of Cl are 0% or more, 0.001% or more, 0.005% or more, 0.008% or more, 0.010% or more, 0.015% or more, 0.018% or more, and 0.
  • the alkali metal oxide is an ion exchange component, which is a component that lowers the high-temperature viscosity and enhances meltability and moldability. If the content of the alkali metal oxide ([Li 2 O] + [Na 2 O] + [K 2 O]) is too large, the coefficient of thermal expansion may increase. In addition, acid resistance may decrease. Therefore, the suitable lower limit range of the alkali metal oxide ([Li 2 O] + [Na 2 O] + [K 2 O]) is 10% or more, 11% or more, 12% or more, 13% or more, 14% or more.
  • the preferred upper limit range of the alkali metal oxide is 25% or less, 23% or less, 20% or less, 19% or less, 18% or less. Is.
  • Molar ratio ([SiO 2 ] +1.2 x [P 2 O 5 ] -3 x [Al 2 O 3 ]-[B 2 O 3 ] -2 x [Li 2 O] -1.5 x [Na 2 O] ]-[K 2 O]) is preferably -40% or more, -30% or more, -25% or more, -24% or more, -23% or more, -22% or more, -21% or more, -20%. As mentioned above, it is -19% or more, especially -18% or more.
  • the molar ratio ([SiO 2 ] + 1.2 ⁇ [P 2 O 5 ] -3 ⁇ [Al 2 O 3 ]-[B 2 O 3 ] -2 ⁇ [Li 2 O] -1.5 ⁇ [Na 2 O]-[K 2 O]) is preferably 30% or less, 20% or less, 15% or less, 10% or less, 5% or less, and particularly 0% or less.
  • molar ratio ([SiO 2 ] + 1.2 ⁇ [P 2 O 5 ] -3 ⁇ [Al 2 O 3 ]-[B 2 O 3 ] -2 ⁇ [Li 2 O] -1.5 ⁇ [ "Na 2 O]-[K 2 O])" is 3 times the content of Al 2 O 3 from the sum of the content of SiO 2 and 1.5 times the content of P 2 O 5 , B. It is obtained by subtracting the total amount of 2 O 3 content, Li 2 O content twice, Na 2 O content 1.5 times, and K 2 O content.
  • CaO is a component that lowers high-temperature viscosity, enhances meltability and moldability, and enhances strain points and Vickers hardness without lowering devitrification resistance as compared with other components.
  • the preferred upper limit range of CaO is 6% or less, 5% or less, 4% or less, 3.5% or less, 3% or less, 2% or less, 1% or less, less than 1%, 0.7% or less, 0. It is 5.5% or less, 0.3% or less, 0.1% or less, 0.05% or less, especially 0.01% or less.
  • SrO and BaO are components that lower the high-temperature viscosity, improve the meltability and moldability, and increase the strain point and Young's modulus, but if their contents are too large, the ion exchange reaction is likely to be inhibited. In addition, the density and coefficient of thermal expansion become unreasonably high, and the glass tends to be devitrified. Therefore, the suitable contents of SrO and BaO are 0 to 2%, 0 to 1.5%, 0 to 1%, 0 to 0.5%, 0 to 0.1%, and particularly 0 to 0.1, respectively. Less than%.
  • ZnO is a component that enhances ion exchange performance, and is a component that has a particularly large effect of increasing the compressive stress value on the outermost surface. It is also a component that lowers the high temperature viscosity without lowering the low temperature viscosity. Suitable lower limit ranges of ZnO are 0% or more, 0.1% or more, 0.3% or more, 0.5% or more, 0.7% or more, and particularly 1% or more. On the other hand, if the ZnO content is too high, the glass tends to be phase-separated, the devitrification resistance is lowered, the density is high, and the stress depth is shallow.
  • suitable upper limit ranges of ZnO are 10% or less, 6% or less, 5% or less, 4% or less, 3% or less, 2% or less, 1.5% or less, 1.3% or less, 1.2% or less. Especially, it is 1.1% or less.
  • ZrO 2 is a component that enhances Vickers hardness and a component that enhances viscosity and strain points near the liquid phase viscosity, but if the content is too large, the devitrification resistance may be significantly lowered. Therefore, the suitable content of ZrO 2 is 0 to 3%, 0 to 1.5%, 0-1%, and particularly 0 to 0.1 mol%.
  • TiO 2 is a component that enhances ion exchange performance and a component that lowers high-temperature viscosity, but if the content thereof is too large, transparency and devitrification resistance tend to decrease. Therefore, the suitable content of TiO 2 is 0 to 3%, 0 to 1.5%, 0 to 1%, 0 to 0.1%, and particularly 0.001 to 0.1 mol%.
  • 0.001 to 1 mol% of one or more selected from the group of SO 3 and CeO 2 (preferably the group of SO 3 ) may be added.
  • Fe 2 O 3 is an impurity that is inevitably mixed from the raw material. Suitable contents of Fe 2 O 3 are 1000 ppm or less (0.1% or less), less than 800 ppm, less than 600 ppm, less than 400 ppm, and particularly less than 300 ppm. If the content of Fe 2 O 3 is too large, the transmittance of the cover glass tends to decrease. On the other hand, the lower limit range is 10 ppm or more, 20 ppm or more, 30 ppm or more, 50 ppm or more, 80 ppm or more, and 100 ppm or more. If the content of Fe 2 O 3 is too small, a high-purity raw material is used, so that the raw material cost rises and the product cannot be manufactured at low cost.
  • Rare earth oxides such as Nd 2 O 3 , La 2 O 3 , Y 2 O 3 , Nb 2 O 5 , Ta 2 O 5 , and Hf 2 O 3 are components that increase Young's modulus.
  • the raw material cost is high, and if a large amount is added, the devitrification resistance tends to decrease. Therefore, the suitable content of the rare earth oxide is 5% or less, 4% or less, 3% or less, 2% or less, 1% or less, 0.5% or less, and particularly 0.1 mol% or less.
  • the tempered glass plate (tempered glass plate) of the present invention preferably contains substantially no As 2 O 3 , Sb 2 O 3 , PbO, and F as a glass composition. Further, from the viewpoint of environmental consideration, it is also preferable that Bi 2 O 3 is not substantially contained. "Substantially free of " means that although the explicit component is not positively added as a glass component, the addition of an impurity level is permitted. Specifically, the content of the explicit component is 0. Refers to the case of less than 0.05%.
  • the tempered glass plate (tempered glass plate) of the present invention preferably has the following characteristics.
  • the density is preferably 2.55 g / cm 3 or less, 2.53 g / cm 3 or less, 2.50 g / cm 3 or less, 2.49 g / cm 3 or less, 2.45 g / cm 3 or less, especially 2.35 to. It is 2.44 g / cm 3 .
  • the coefficient of thermal expansion at 30 to 380 ° C. is preferably 150 ⁇ 10 -7 / ° C. or less, 100 ⁇ 10 -7 / ° C. or less, and particularly 50 to 95 ⁇ 10 -7 / ° C.
  • the "coefficient of thermal expansion at 30 to 380 ° C.” refers to a value obtained by measuring the average coefficient of thermal expansion using a dilatometer.
  • the softening points are preferably 950 ° C or lower, 940 ° C or lower, 930 ° C or lower, 920 ° C or lower, 910 ° C or lower, 900 ° C or lower, 890 ° C or lower, 880 ° C or lower, 870 ° C or lower, 860 ° C or lower, 850 ° C or lower, 840 ° C or lower, 830 ° C or lower, particularly 820 to 700 ° C.
  • the "softening point” refers to a value measured based on the method of ASTM C338.
  • the temperature at a high temperature viscosity of 10 2.5 dPa ⁇ s is preferably 1680 ° C or lower, 1680 ° C or lower, 1670 ° C or lower, 1660 ° C or lower, 1650 ° C or lower, 1640 ° C or lower, 1630 ° C or lower, 1620 ° C or lower, 1600 ° C or lower. In particular, 1400 to 1590 ° C. is preferable. If the temperature at a high temperature viscosity of 10 2.5 dPa ⁇ s is too high, the meltability and moldability deteriorate, and it becomes difficult to mold the molten glass into a plate shape.
  • the “temperature at a high temperature viscosity of 10 2.5 dPa ⁇ s” refers to a value measured by the platinum ball pulling method.
  • the liquidus viscosity is preferably 10 3.74 dPa ⁇ s or higher, 10 4.5 dPa ⁇ s or higher, 10 4.8 dPa ⁇ s or higher, 10 4.9 dPa ⁇ s or higher, and 10 5.0 dPa ⁇ s. 10 5.1 dPa ⁇ s or more, 10 5.2 dPa ⁇ s or more, 10 5.3 dPa ⁇ s or more, 10 5.4 dPa ⁇ s or more, especially 10 5.5 dPa ⁇ s or more.
  • the higher the liquidus viscosity the better the devitrification resistance, and the less likely it is that devitrification will occur during molding.
  • liquid phase viscosity refers to a value obtained by measuring the viscosity at the liquid phase temperature by the platinum ball pulling method.
  • “Liquid phase temperature” means that the glass powder that has passed through a standard sieve of 30 mesh (500 ⁇ m) and remains in 50 mesh (300 ⁇ m) is placed in a platinum boat, held in a temperature gradient furnace for 24 hours, and then the platinum boat is taken out. The highest temperature at which devitrification (devitrification) was observed inside the glass by microscopic observation.
  • Young's modulus is preferably 70 GPa or more, 74 GPa or more, 75 to 100 GPa, and particularly 76 to 90 GPa. When the Young's modulus is low, the cover glass tends to bend when the plate thickness is thin.
  • the "Young's modulus" can be calculated by a well-known resonance method.
  • the tempered glass plate of the present invention has a compressive stress layer on the surface.
  • the compressive stress value on the outermost surface is preferably 165 MPa or more, 200 MPa or more, 220 MPa or more, 250 MPa or more, 280 MPa or more, 300 MPa or more, 310 MPa or more, and particularly 320 MPa or more.
  • the larger the compressive stress value on the outermost surface the higher the Vickers hardness.
  • the tensile stress inherent in the tempered glass becomes extremely high, and there is a possibility that the dimensional change before and after the ion exchange treatment becomes large.
  • the compressive stress value on the outermost surface is preferably 1200 MPa or less, 1100 MPa or less, 1000 MPa or less, 900 MPa or less, 700 MPa or less, 680 MPa or less, 650 MPa or less, and particularly 600 MPa or less. If the ion exchange time is shortened or the temperature of the ion exchange solution is lowered, the compressive stress value on the outermost surface tends to increase.
  • the stress depth is preferably 50 ⁇ m or more, 60 ⁇ m or more, 80 ⁇ m or more, 100 ⁇ m or more, and particularly 120 ⁇ m or more.
  • the deeper the stress depth the more difficult it is for protrusions and sand particles on the road surface to reach the tensile stress layer when the smartphone is dropped, and it becomes possible to reduce the probability of damage to the cover glass.
  • the stress depth is too deep, there is a risk that the dimensional change will be large before and after the ion exchange treatment. Further, the compressive stress value on the outermost surface tends to decrease. Therefore, the stress depth is preferably 200 ⁇ m or less, 180 ⁇ m or less, 150 ⁇ m or less, and particularly 140 ⁇ m or less. If the ion exchange time is lengthened or the temperature of the ion exchange solution is raised, the stress depth tends to increase.
  • the plate thickness is preferably 2.0 mm or less, 1.5 mm or less, 1.3 mm or less, 1.1 mm or less, 1.0 mm or less, 0.9 mm or less, particularly 0.8 mm or less. be.
  • the plate thickness is preferably 0.1 mm or more, 0.3 mm or more, 0.4 mm or more, 0.5 mm or more, 0.6 mm or more, and particularly 0.7 mm or more.
  • the method for producing a reinforced glass plate of the present invention has a glass composition of SiO 2 55 to 80%, Al 2 O 3 11 to 25%, B 2 O 30 to 10%, and Li 2 O 0.02 in terms of glass composition. Containing ⁇ 15%, Na 2 O 1 ⁇ 21%, K 2 O 0 ⁇ 10%, MgO 0.01 ⁇ 5 %, P 2 O 50 ⁇ 15%, SnO 20 ⁇ 0.30%, mol
  • the method for manufacturing a tempered glass plate of the present invention is characterized in that it is subjected to a plurality of ion exchange treatments, but the tempered glass plate of the present invention is only subjected to a plurality of ion exchange treatments. However, it also includes the case where the ion exchange treatment is performed only once.
  • the method for manufacturing the tempering glass is as follows. First, a glass raw material prepared to have a desired glass composition is put into a continuous melting furnace, heated and melted at 1400 to 1700 ° C., clarified, and then the molten glass is supplied to a molding apparatus and molded into a plate shape. , It is preferable to cool.
  • a well-known method can be adopted as a method of cutting into a predetermined size after forming into a plate shape.
  • the overflow down draw method is preferable as a method for forming the molten glass into a plate shape.
  • the surface of the glass plate which should be the surface, does not come into contact with the surface of the refractory molded body, and is formed into a plate shape with a free surface. Therefore, it is possible to inexpensively manufacture a glass plate having a good surface quality while being unpolished.
  • an alumina-based refractory or a zirconia-based refractory is used as the refractory of the molded body.
  • the tempered glass plate (tempered glass plate) of the present invention has good compatibility with alumina-based refractories and zirconia-based refractories (particularly alumina-based refractories), and therefore reacts with these refractories. It has the property that it is difficult to generate bubbles and lumps.
  • a forming method such as a float method, a down draw method (slot down draw method, redraw method, etc.), a rollout method, a press method, etc. can be adopted.
  • the temperature range between the slow cooling point and the strain point of the molten glass it is preferable to cool the temperature range between the slow cooling point and the strain point of the molten glass at a cooling rate of 3 ° C./min or more and less than 1000 ° C./min, and the lower limit range of the cooling rate is It is preferably 10 ° C./min or more, 20 ° C./min or more, 30 ° C./min or more, particularly 50 ° C./min or more, and the upper limit range is preferably less than 1000 ° C./min, less than 500 ° C./min, especially 300. Less than ° C / min. If the cooling rate is too fast, the structure of the glass becomes rough and it becomes difficult to increase the Vickers hardness after the ion exchange treatment. On the other hand, if the cooling rate is too slow, the production efficiency of the glass plate will decrease.
  • ion exchange treatment is performed a plurality of times.
  • a plurality of ion exchange treatments it is preferable to perform an ion exchange treatment of immersing in a molten salt containing a KNO 3 molten salt and then an ion exchange treatment of immersing in a molten salt containing a NaNO 3 molten salt.
  • KNO 3 and LiNO 3 are used.
  • second ion exchange step an ion exchange treatment of immersing in the mixed molten salt.
  • a stress profile that is bent in the thickness direction.
  • the non-monotonic stress profile shown in FIG. 1 that is, a stress profile having at least a first peak, a second peak, a first bottom, and a second bottom can be formed. As a result, it becomes possible to significantly reduce the probability of damage to the cover glass when the smartphone is dropped.
  • Li ions contained in the glass and Na ions in the molten salt are ion-exchanged, and when a NaNO 3 and KNO 3 mixed molten salt is used, the Na ions contained in the glass and the molten salt are further exchanged.
  • the K ions inside exchange ions Here, the ion exchange between the Li ion contained in the glass and the Na ion in the molten salt is faster than the ion exchange between the Na ion contained in the glass and the K ion in the molten salt, and the ion exchange efficiency is high. high.
  • Na ions in the vicinity of the glass surface (shallow region from the outermost surface to 20% of the plate thickness) and Li ions in the molten salt exchange ions, and in addition, near the glass surface (from the outermost surface to the plate).
  • Na ions in the shallow region up to 20% of the thickness and K ions in the molten salt exchange ions. That is, in the second ion exchange step, K ions having a large ionic radius can be introduced while separating Na ions in the vicinity of the glass surface. As a result, the compressive stress value on the outermost surface can be increased while maintaining a deep stress depth.
  • the temperature of the molten salt is preferably 360 to 400 ° C., and the ion exchange time is preferably 30 minutes to 6 hours.
  • the temperature of the ion exchange solution is preferably 370 to 400 ° C., and the ion exchange time is preferably 15 minutes to 3 hours.
  • the concentration of NaNO 3 is preferably higher than the concentration of KNO 3
  • the concentration of KNO 3 is more than 0% by mass, preferably 0.5% by mass or more, preferably 1% by mass or more, 5% by mass or more, and 7% by mass. % Or more, 10% by mass or more, 15% by mass or more, particularly 20 to 90% by mass. If the concentration of KNO 3 is too high, the compressive stress value formed when the Li ion contained in the glass and the Na ion in the molten salt exchange ions may be too low. Further, if the concentration of KNO 3 is too low, it may be difficult to measure the stress with the surface stress meter FSM-6000.
  • the concentration of LiNO 3 is preferably more than 0 to 5% by mass, more than 0 to 3% by mass, more than 0 to 2% by mass, and particularly 0. It is 1 to 1% by mass. If the concentration of LiNO 3 is too low, it becomes difficult for Na ions to escape in the vicinity of the glass surface. On the other hand, if the concentration of LiNO 3 is too high, the compressive stress value formed by ion exchange between Na ions and K ions in the molten salt near the glass surface may decrease too much.
  • Table 1 shows the glass composition and glass properties of Examples (Samples Nos. 1 to 6, 9, and 10) and Comparative Examples (Samples Nos. 7 and 8) of the present invention.
  • "NA" means unmeasured
  • (Li + Na + K) / Al is the molar ratio ([Li 2 O] + [Na 2 O] + [K 2 O]) / [ It means Al 2 O 3 ]
  • Mg / Al means a molar ratio [MgO] / [Al 2 O 3 ].
  • Each sample in the table was prepared as follows. First, glass raw materials were prepared so as to have the glass composition shown in the table, and melted at 1600 ° C. for 21 hours using a platinum pot. Subsequently, the obtained molten glass was poured onto a carbon plate to form a flat plate, and then the temperature range between the slow cooling point and the strain point was cooled at 3 ° C./min to make a glass plate (for strengthening). Glass plate) was obtained. The surface of the obtained glass plate was optically polished so that the plate thickness was 1.5 mm, and then various characteristics were evaluated.
  • each glass is cut into an appropriate size, placed in a platinum boat together with an alumina refractory having the same composition as the molded refractory, and kept in a temperature gradient furnace for 48 hours. After that, the platinum boat was taken out, and microscopic observation was performed on the part held at a temperature of 10 4.5 dPa ⁇ s or higher. " ⁇ " and those that were not recognized were marked as " ⁇ ".
  • Density is a value measured by the well-known Archimedes method.
  • the coefficient of thermal expansion (CTE 30-380 ° C. ) at 30 to 380 ° C. is a value obtained by measuring the average coefficient of thermal expansion using a dilatometer.
  • the softening point is a value measured based on the method of ASTM C338.
  • the temperature at a high temperature viscosity of 10 2.5 dPa ⁇ s is a value measured by the platinum ball pulling method.
  • sample No. In Nos. 7 and 8 since the molar ratio [MgO] / [Al 2 O 3 ] was larger than 0.20, devitrification with the refractory of the molded body was observed.
  • the glass thus obtained is subjected to, for example, an ion exchange treatment of immersing it in a molten salt containing a KNO 3 molten salt and then an ion exchange treatment of immersing it in a molten salt containing a NaNO 3 molten salt. ,
  • the tempered glass of the present invention can be obtained.
  • the tempered glass plate of the present invention is suitable as a cover glass for a touch panel display of a mobile phone, a digital camera, a PDA (mobile terminal) or the like.
  • the tempered glass plate of the present invention is used for applications requiring high mechanical strength, such as window glass, magnetic disk substrates, flat panel display substrates, flexible display substrates, and solar cells. It is expected to be applied to cover glass, cover glass for solid-state image pickup elements, and cover glass for automobiles.

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Abstract

La présente invention concerne une plaque de verre renforcée qui a une couche de contrainte de compression sur sa surface, et est caractérisée en ce qu'elle a une composition de verre contenant, sur une base molaire, de 55 à 80% de SiO2, de 11 à 25% d'Al2O3, de 0,4 à 10% de B2O3, de 0,02 à 15% de Li2O, de 1 à 21% de Na2O, de 0 à 10% de K2O, de 0,01 à 5% de MgO, de 0 à 15% de P2O5, et de 0 à 0,30% de SnO2%, et ayant un rapport molaire [MgO]/[Al2O3] ≤ 0,20 et un rapport molaire ([Li2O] + [Na2O] + [K2O])/[Al2O3] ≥ 0,80.
PCT/JP2021/047907 2020-12-29 2021-12-23 Plaque de verre renforcée et procédé de production associé WO2022145340A1 (fr)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
JP2013536155A (ja) * 2010-08-26 2013-09-19 コーニング インコーポレイテッド ガラスを強化する二段階法
JP2019031428A (ja) * 2017-08-08 2019-02-28 日本電気硝子株式会社 強化ガラス板及び強化ガラス球
WO2020075709A1 (fr) * 2018-10-09 2020-04-16 日本電気硝子株式会社 Verre renforcé et procédé de production de verre renforcé
WO2020138062A1 (fr) * 2018-12-25 2020-07-02 日本電気硝子株式会社 Vitre trempée est son procédé de fabrication

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JP2006083045A (ja) 2004-09-17 2006-03-30 Hitachi Ltd ガラス部材
CN101939267B (zh) 2008-02-08 2014-09-17 康宁股份有限公司 抗损伤的、化学钢化的防护性盖板玻璃
US9110230B2 (en) 2013-05-07 2015-08-18 Corning Incorporated Scratch-resistant articles with retained optical properties

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013536155A (ja) * 2010-08-26 2013-09-19 コーニング インコーポレイテッド ガラスを強化する二段階法
JP2019031428A (ja) * 2017-08-08 2019-02-28 日本電気硝子株式会社 強化ガラス板及び強化ガラス球
WO2020075709A1 (fr) * 2018-10-09 2020-04-16 日本電気硝子株式会社 Verre renforcé et procédé de production de verre renforcé
WO2020138062A1 (fr) * 2018-12-25 2020-07-02 日本電気硝子株式会社 Vitre trempée est son procédé de fabrication

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